CN110568026A - cobalt oxide nano-sheet gas sensor and preparation method thereof - Google Patents
cobalt oxide nano-sheet gas sensor and preparation method thereof Download PDFInfo
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- CN110568026A CN110568026A CN201910909551.2A CN201910909551A CN110568026A CN 110568026 A CN110568026 A CN 110568026A CN 201910909551 A CN201910909551 A CN 201910909551A CN 110568026 A CN110568026 A CN 110568026A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a cobalt oxide nano-sheet gas sensor and a preparation method thereof, relating to the technical field of gas sensing material preparation and comprising a sensor and a preparation method thereof; the sensor is of a nano flaky structure with the transverse size of 1-3 mu m and the thickness of 1-5 nm, and comprises cobalt element, oxygen element and cadmium element, wherein the atomic ratio of the content of the cadmium element is 1% -9%; mixing the cobalt ions, the cadmium ions, urea and ethylene glycol in a solution, obtaining a cobalt hydroxide nanosheet precursor through microwave hydrothermal reaction, then dropwise adding a sensing material onto the interdigital electrode, and converting the cobalt hydroxide nanosheet precursor into a cobalt oxide nanosheet through high-temperature annealing, thereby preparing the sensor. Compared with the prior art, the technical scheme disclosed by the invention has the advantages that the raw materials used in the preparation process are wide in source and low in cost, and the prepared sensor has high response speed and good repeatability under the room temperature condition.
Description
Technical Field
the invention belongs to the technical field of preparation of gas sensing materials, relates to a material of a gas sensor and a preparation method thereof, and particularly relates to a cadmium-doped cobalt oxide nanosheet gas sensor and a preparation method thereof.
Background
With the rapid development of economic science and technology and the increasing promotion of urbanization, the requirements of people on the living quality and self health are increased. However, the problem of air pollution in China is still very serious at present, and nitrogen oxides (NO and NO) caused by exhaust gas of motor vehicles and exhaust gas of factories are discharged2And N2O3Etc.) contamination is on an increasing trend. Wherein nitrogen dioxide (NO)2) Is one of the most harmful gases to the human body, and has a low concentration of NO of about 1ppm (parts per million)2It may irritate the nose, eyes and throat of the human body. More seriously, prolonged exposure to certain concentrations of NO2The chances of respiratory infections and lung disease are increased. Thus, real-time fast NO for public safety and personal safety2The development of a highly sensitive gas sensor for detection is an urgent need.
In practical applications, the resistance-sensitive semiconductor gas sensor is the most widely used. Through controllable preparation of the nano semiconductor material, shape adjustment and self-assembly of the multilevel structure, the defect of high working temperature of the traditional sensing material can be overcome to a greater extent, and the nano gas sensor has more sensitive and reliable detection performance and lower power consumption. Based on Metal Oxide Semiconductors (MOS), e.g. SnO2、ZnO、α-Fe2O3、In2O3、CuO、Co3O4NiO and the like, and is widely applied to trace NO due to the advantages of low production cost, good stability, wide application range, easy integration and the like2and can be easily integrated with a portable device for assembly and use.
The traditional metal oxide semiconductor-based resistance-sensitive gas sensor works in a high-temperature environment, and although the sensitivity of the traditional metal oxide semiconductor-based resistance-sensitive gas sensor is greatly improved, extra energy consumption is increased. In recent years, with the development of nanotechnology, modifications to nanomaterials themselves, such as: the method of element doping, semiconductor compounding, noble metal modification and the like greatly improves the performance of the nano semiconductor sensing material, and the room-temperature gas sensor becomes possible. However, at room temperature, the gas sensor with high response has the defects of slow recovery, poor cycle performance and the like.
Therefore, those skilled in the art are dedicated to develop a gas sensor, which has the advantages of high room temperature detection sensitivity, good recovery, excellent selectivity, simple manufacturing process, controllable cost, and low possibility of damage.
Disclosure of Invention
in view of the above-mentioned defects in the prior art, the technical problem to be solved by the present invention is to provide a gas sensing material and a device manufacturing method, which have high response to low-concentration nitrogen dioxide gas at room temperature and fast recovery performance, aiming at the situation that detection accuracy, manufacturing cost, process complexity and the like in the prior art cannot be considered at the same time.
In order to achieve the purpose, the invention provides a cobalt oxide nanosheet gas sensor and a preparation method thereof. The specific technical scheme is as follows:
The invention discloses a cobalt oxide nano-sheet gas sensor.
further, the sensor is a nano sheet-like structure with the transverse dimension of 1-3 mu m and the thickness of 1-5 nm.
Further, the sensor comprises cobalt element, oxygen element and cadmium element, and the atomic ratio of the content of the cadmium element is 1-9%.
The invention also discloses a preparation method of the cobalt oxide nanosheet gas sensor, which comprises the following steps:
Dissolving soluble cobalt salt, soluble cadmium salt and urea in water to form a first mixed solution; the concentration of the soluble cobalt salt in the first mixed solution is 0.01-0.2 mol/L; the molar weight ratio of the soluble cadmium salt to the soluble cobalt salt in the first mixed solution is 1: 10-1: 100; the concentration of the urea in the first mixed solution is 0.04-0.8 mol/L.
And step two, adding ethylene glycol into the first mixed solution, and stirring and mixing uniformly to form a second mixed solution.
and step three, adding the second mixed solution into a microwave hydrothermal reaction bottle, and carrying out microwave hydrothermal reaction to obtain the cobalt hydroxide nanosheet.
and step four, centrifugally washing the cobalt hydroxide nanosheets to remove impurities, and dissolving the cobalt hydroxide nanosheets in absolute ethyl alcohol to form a third mixed solution.
And fifthly, after the third mixed solution is subjected to ultrasonic treatment, the third mixed solution is dripped on the interdigital electrode, and the third mixed solution is naturally volatilized at room temperature to form uniformly distributed film materials.
And sixthly, annealing the whole film material to obtain the cadmium-doped cobalt oxide nanosheet gas sensor.
Further, the soluble cobalt salt is selected from any one of cobalt acetate tetrahydrate, cobalt chloride or cobalt nitrate hexahydrate.
Further, the soluble cadmium salt is cadmium chloride or cadmium nitrate.
Further, the volume ratio of the added glycol to the first mixed solution is 9: 1-1: 1.
Further, the stirring time in the second step is 0.05-0.3 h.
Further, in the third step, the temperature of the microwave hydrothermal reaction is 120-180 ℃, and the heat preservation time of the microwave hydrothermal reaction is 0.3-1 h.
Further, in the fourth step, a dispersing solvent used in the centrifugal washing process is ethanol, and the dispersed concentration of the cobalt hydroxide is 0.01-0.1 mol/L.
Further, the ultrasonic treatment time in the fifth step is 0.2-0.8 h.
Further, in the sixth step, the annealing temperature is 350-550 ℃, and the annealing treatment time is 2-10 hours.
Compared with the prior art, the method has the advantages of wide raw material source and low cost.
The nitrogen dioxide gas sensor obtained by the invention has high response speed and good repeatability under the room temperature condition.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a flow chart of the fabrication of a cobalt oxide nanosheet gas sensor in accordance with a preferred embodiment of the present invention;
FIG. 2 is a SEM photograph of the electrode and the adhesion material of the gas sensor prepared according to the preferred embodiment of the present invention;
FIG. 3 is a scanning electron micrograph of a gas sensor material prepared in accordance with a preferred embodiment of the present invention;
FIG. 4 is an X-ray diffraction pattern of a gas sensor material prepared according to a preferred embodiment of the present invention;
FIG. 5 is a graph of the complete response of a gas sensor made in accordance with a preferred embodiment of the present invention;
FIG. 6 is a graph of the repeatability of a gas sensor made in accordance with a preferred embodiment of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific embodiments. It should be understood that the embodiments are illustrative of the invention and are not to be construed as limiting the scope of the invention in any way. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
Example 1:
step one, dissolving 47.6mg of cobalt chloride hexahydrate, 48.0mg of urea and 18.4mg of cadmium chloride in 10mL of deionized water, and fully stirring to completely dissolve to form a first uniformly dispersed mixed solution.
And step two, adding 10mL of glycol solution into the first mixed solution, and stirring for 5min to uniformly mix the solution to form a second mixed solution.
And step three, transferring the second mixed solution into a microwave reaction kettle, heating to 150 ℃ for microwave hydrothermal reaction, preserving heat for 20min to obtain the cobalt hydroxide nanosheet, taking out and transferring into a centrifuge tube.
And step four, respectively centrifuging and washing the product obtained in the step three for 3 times by using deionized water and ethanol, setting the rotating speed of a centrifuge to 6500r/min, and centrifuging for 5min each time. Dispersing the obtained cobalt hydroxide nano-flakes in absolute ethyl alcohol to form a light red transparent liquid, namely a third mixed solution.
And fifthly, taking 2 mu L of the third mixed solution, carrying out ultrasonic treatment for 20min, dripping the third mixed solution on the interdigital electrode, and forming a layer of uniformly distributed film on the electrode after the liquid is completely naturally volatilized at room temperature.
And step six, putting the product of the step five into a muffle furnace, heating to 350 ℃, keeping the temperature, annealing for 2 hours, and taking out after naturally cooling to room temperature. And (4) mounting the annealed sensor on a special base, and connecting the electrode with a binding post by using an aluminum wire machine.
fig. 1 is a flowchart of a process for preparing a cobalt oxide nanosheet gas sensor according to this embodiment, and it can be seen from the flowchart that the technical scheme disclosed by the present invention is simple in process and easy to implement in the sensor preparation process.
fig. 2 is a scanning electron micrograph of the gas sensor electrode and the adhesive material prepared in this example, and it can be seen from the micrograph that the gas sensor material is uniformly coated on the interdigital electrode.
FIG. 3 is a scanning electron microscope photograph of the gas sensor material prepared in this embodiment, from which it can be seen that the prepared cobalt oxide has a flake structure, a lateral dimension of 1-3 μm, and a thickness of 1-5 nm.
Fig. 4 is an X-ray diffraction spectrum of the gas sensor material prepared in this example, and it can be seen from the spectrum that the prepared sample is a pure-phase cobalt oxide material.
Fig. 5 is a graph of the complete response of the gas sensor prepared in this embodiment, and it can be seen that the gas sensor prepared in this embodiment has good gas sensing performance.
Fig. 6 is a graph of the repeatability of the gas sensor prepared in this example, and it can be seen that the gas sensing performance of the prepared sensor has excellent repeatability.
Example 2:
Step one, dissolving 47.6mg of cobalt chloride hexahydrate, 48.0mg of urea and 11.0mg of cadmium chloride in 10mL of deionized water, and fully stirring to completely dissolve to form a first uniformly dispersed mixed solution.
And step two, adding 10mL of glycol solution into the first mixed solution, and stirring for 7min to uniformly mix the solution to form a second mixed solution.
And step three, transferring the second mixed solution into a microwave reaction kettle, heating to 160 ℃ for microwave hydrothermal reaction, keeping the temperature for 25min to prepare the cobalt hydroxide nanosheet, taking out the cobalt hydroxide nanosheet and transferring the cobalt hydroxide nanosheet into a centrifuge tube.
And step four, respectively centrifuging and washing the product obtained in the step three for 4 times by using deionized water and ethanol, setting the rotating speed of a centrifuge to be 6000r/min, and centrifuging for 5min each time. Dispersing the obtained cobalt hydroxide nano-flakes in absolute ethyl alcohol to form a light red transparent liquid, namely a third mixed solution.
And fifthly, taking 2 mu L of the third mixed solution, carrying out ultrasonic treatment for 30min, dripping the third mixed solution on the interdigital electrode, and forming a layer of uniformly distributed film on the electrode after the liquid is completely naturally volatilized at room temperature.
And step six, putting the product obtained in the step five into a muffle furnace, heating to 400 ℃, keeping the temperature, cooling for 5 hours, and taking out after naturally cooling to room temperature. And (4) mounting the annealed sensor on a special base, and connecting the electrode with a binding post by using an aluminum wire machine.
Example 3:
step one, dissolving 47.6mg of cobalt chloride hexahydrate, 24.0mg of urea and 25.7mg of cadmium chloride in 10mL of deionized water, and fully stirring to completely dissolve to form a first uniformly dispersed mixed solution.
And step two, adding 10mL of glycol solution into the first mixed solution, and stirring for 5min to uniformly mix the solution to form a second mixed solution.
And step three, transferring the second mixed solution into a microwave reaction kettle, heating to 150 ℃ for microwave hydrothermal reaction, preserving heat for 20min to obtain the cobalt hydroxide nanosheet, taking out and transferring into a centrifuge tube.
And step four, respectively centrifuging and washing the product obtained in the step three for 3 times by using deionized water and ethanol, setting the rotating speed of a centrifuge to 6500r/min, and centrifuging for 4min each time. Dispersing the obtained cobalt hydroxide nano-flakes in absolute ethyl alcohol to form a light red transparent liquid, namely a third mixed solution.
And fifthly, taking 2 mu L of the third mixed solution, carrying out ultrasonic treatment for 35min, dripping the third mixed solution on the interdigital electrode, and forming a layer of uniformly distributed film on the electrode after the liquid is completely naturally volatilized at room temperature.
and step six, putting the product of the step five into a muffle furnace, heating to 450 ℃, keeping the temperature, annealing for 4 hours, and taking out after naturally cooling to room temperature. And (4) mounting the annealed sensor on a special base, and connecting the electrode with a binding post by using an aluminum wire machine.
Example 4:
Step one, 23.8mg of cobalt chloride hexahydrate, 24.0mg of urea and 18.4mg of cadmium chloride are dissolved in 10mL of deionized water, and fully stirred to be completely dissolved to form a first mixed solution which is uniformly dispersed.
And step two, adding 10mL of glycol solution into the first mixed solution, and stirring for 5min to uniformly mix the solution to form a second mixed solution.
And step three, transferring the second mixed solution into a microwave reaction kettle, heating to 150 ℃ for microwave hydrothermal reaction, preserving heat for 20min to obtain the cobalt hydroxide nanosheet, taking out and transferring into a centrifuge tube.
And step four, respectively centrifuging and washing the product obtained in the step three for 3 times by using deionized water and ethanol, setting the rotating speed of a centrifuge to 6500r/min, and centrifuging for 4min each time. Dispersing the obtained cobalt hydroxide nano-flakes in absolute ethyl alcohol to form a light red transparent liquid, namely a third mixed solution.
And fifthly, taking 2 mu L of the third mixed solution, carrying out ultrasonic treatment for 35min, dripping the third mixed solution on the interdigital electrode, and forming a layer of uniformly distributed film on the electrode after the liquid is completely naturally volatilized at room temperature.
And step six, putting the product of the step five into a muffle furnace, heating to 550 ℃, keeping the temperature, annealing for 4 hours, and taking out after naturally cooling to room temperature. And (4) mounting the annealed sensor on a special base, and connecting the electrode with a binding post by using an aluminum wire machine.
the foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. the cobalt oxide nanosheet gas sensor is characterized in that the sensor is of a nanosheet structure with a transverse size of 1-3 mu m and a thickness of 1-5 nm;
The sensor comprises cobalt element, oxygen element and cadmium element, wherein the atomic ratio of the content of the cadmium element is 1-9%.
2. The method for preparing a cobalt oxide nanosheet gas sensor of claim 1, comprising the steps of:
Dissolving soluble cobalt salt, soluble cadmium salt and urea in water to form a first mixed solution;
Adding ethylene glycol into the first mixed solution, and stirring and mixing uniformly to form a second mixed solution;
Adding the second mixed solution into a microwave hydrothermal reaction bottle, and carrying out microwave hydrothermal reaction to obtain a cobalt hydroxide nanosheet;
Step four, centrifugally washing the cobalt hydroxide nanosheets to remove impurities, and dissolving the cobalt hydroxide nanosheets in absolute ethyl alcohol to form a third mixed solution;
Step five, after the third mixed solution is subjected to ultrasonic treatment, the third mixed solution is dripped on an interdigital electrode, and a uniformly distributed thin film material is formed after natural volatilization at room temperature;
Sixthly, annealing the whole thin film material to obtain the cadmium-doped cobalt oxide nanosheet gas sensor;
the concentration of the soluble cobalt salt in the first mixed solution is 0.01-0.2 mol/L;
The molar weight ratio of the soluble cadmium salt to the soluble cobalt salt in the first mixed solution is 1: 10-1: 100;
The concentration of the urea in the first mixed solution is 0.04-0.8 mol/L.
3. the method of preparing a cobalt oxide nanosheet gas sensor of claim 2, wherein the soluble cobalt salt is selected from any one of cobalt acetate tetrahydrate, cobalt chloride, or cobalt nitrate hexahydrate.
4. The method of claim 2, wherein the soluble cadmium salt is cadmium chloride or cadmium nitrate.
5. The method for preparing a cobalt oxide nanosheet gas sensor of claim 2, wherein the ratio of the volume of the added ethylene glycol to the volume of the first mixed solution is 9:1 to 1: 1.
6. The method for preparing a cobalt oxide nanosheet gas sensor of claim 2, wherein the stirring time in step two is from 0.05 to 0.3 h.
7. The method for preparing the cobalt oxide nanosheet gas sensor of claim 2, wherein in step three the microwave hydrothermal reaction temperature is 120-180 ℃ and the microwave hydrothermal reaction holding time is 0.3-1 h.
8. The method for preparing a cobalt oxide nanosheet gas sensor of claim 2, wherein the dispersing solvent used in the centrifugal washing in step four is ethanol, and the dispersed concentration of the cobalt hydroxide is 0.01 to 0.1 mol/L.
9. The method for preparing a cobalt oxide nanosheet gas sensor of claim 2, wherein the sonication time in step five is 0.2 to 0.8 h.
10. the method for preparing the cobalt oxide nanosheet gas sensor of claim 2, wherein in step six the annealing temperature is 350 to 550 ℃ and the annealing time is 2 to 10 hours.
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Application publication date: 20191213 |